Bubbleplate (Hive Bee)
09-20-02 07:37
No 358515
      Nitromethane Distillation Safety?  Bookmark   

Just doing a last minute "survey" before the HotPlate/Stirrer gets turned on:

How safe / not safe is it to do a non-vacuum Distillation of say 600 ml of Model Fuel to get the Nitromethane? (Oil bath)
A friend bee says no more dangerous than distilling Methanol.
Another says potentially explosive unless watch temp very carefully.
Also: Yield be damned, wouldn't it be easier/faster to do under even partial vacuum?
Comments, suggestions, experiences?
TIA

If they drive God from the earth, we shall shelter Him underground - Dostoevsky
 
 
 
 
    hest
(Hive Adickt)
09-20-02 08:04
No 358521
      destilation  Bookmark   

Get an wather pump.
In trheory destilation of nitro(m)ethane is explosive, but I have newer heard abouth anny explosions. So I'm sure there is no risk.
 
 
 
 
    Rhodium
(Chief Bee)
09-20-02 08:18
No 358524
      UTFSE  Bookmark   

Read the thread starting with Post 193397 (Rhodium: "Re: Nitromethane distillation probs", Newbee Forum) as well as other posts written by me containing "nitromethane distill".
 
 
 
 
    Diggity
(Hive Bee)
09-20-02 08:46
No 358529
      2 major rules swim followed when he distilled ...  Bookmark   

2 major rules swim followed when he distilled nitro. Do not distill every last drop. Leave some behind with the castor oil you will find. IF you are distilling alot< over 500ml's, change the receiver flask on occasion. Just in case anything does happen, you wont have to wory about the 475ml sitting not far away.

Oh yea, DONT SMOKE, LIGHT YOUR CRACK PIPE, OR USE THE GEORGE FORMAN GRILL ANYWHERE AROUND YOUR RIG.

& I'm, somethin of a phenom, 1 puff of da cron, I'm un-stopable.   
 
 
 
 
 
 
    Bubbleplate
(Hive Bee)
09-20-02 10:03
No 358532
      So If I have "50%" Fuel  Bookmark   

And I'm distilling 600ml, you're saying stop distilling when I have 250 ml, rather than go to 300ml. OK.
Nother question: Oil bath temp read 190 C. But inside the Stillhead the thermometer was reading only 67 C. Lots of clear liquid distilling over, but was that just Methanol?
Shouldn't the temp spike up to 102 for Nitro to come over???

If they drive God from the earth, we shall shelter Him underground - Dostoevsky
 
 
 
 
    Rhodium
(Chief Bee)
09-20-02 10:33
No 358535
      Azeotrope  Bookmark   

Methanol and nitromethane forms an azeotrope that boils at 64.5C, and consists of 92% methanol and 8% nitromethane, therefore, removing the methanol by washing with water as directed in the thread above is reccommended before distillation.
 
 
 
 
    GOD
(Hive Addict)
09-20-02 11:08
No 358542
      bubbleplate  Bookmark   

after distillation:
Post 269664 (Chromic: "Re: 30% nitro methane", Chemicals & Equipment)
Post 270026 (Chromic: "Re: 30% nitro methane", Chemicals & Equipment)
take those #'s and %, and plot them out, then put in a line of best fit.  Get your sg, and then extrapolate from the chart (to find %nitro v/v).



 
 
 
 
    Bubbleplate
(Hive Bee)
09-20-02 12:16
No 358570
      This IS Frustrating!  Bookmark   

Everything else before this (oil distill, Wacker) has been a cakewalk compared to getting Nitromethane!
I guess I'll try washing Fuel with dH2O first, then distilling.
However... I did straight distill 600 ml 50% Fuel and got 250 ml clear liquid. Using TFSE, I saw a post by Baal, so I tried washing the 250ml with 250 dH2O in a sep funnel. Now I have 240 ml of what looks like H2O (on bottom), and maybe 10 ml of a very refractive liquid on top! So now what the hell do I have and do with it???

If they drive God from the earth, we shall shelter Him underground - Dostoevsky
 
 
 
 
    terbium
(Old P2P Cook)
09-20-02 12:22
No 358573
      Azeotrope  Bookmark   

However... I did straight distill 600 ml 50% Fuel and got 250 ml clear liquid.
This should be the azeotrope than contains mostly methanol.

Using TFSE, I saw a post by Baal, so I tried washing the 250ml with 250 dH2O in a sep funnel. Now I have 240 ml of what looks like H2O (on bottom), and maybe 10 ml of a very refractive liquid on top!
Doesn't seem like washing methanol works very well.
 
 
 
 
    Diggity
(Hive Bee)
09-20-02 13:51
No 358588
      bubble.. this is really very easy.  Bookmark   

bubble.. this is really very easy.

I used to distill this shit for my RC cars.. all I did was set the oil bath temp to 95c and come back in a few hours and meoh, and azeotrope will have filled the reciever, nothing else coming over, got it all. Cranked the heat up a little, soon the thermo read 101c.. nitro. Collect 30 drops, add back to fuel bottle, change with a clean new flask, collect close/too pure nitro. Really quiet easy. And not dangerous.

& I'm, somethin of a phenom, 1 puff of da cron, I'm un-stopable.   
 
 
 
 
 
 
    baalchemist
(Chef d'Equippe)
09-20-02 13:52
No 358589
      When Baal was using that 60% blended crap, you ...  Bookmark   

When Baal was using that 60% blended crap, you have to distill off all the MeOH/Nitro, then give that a quick wash to remove the MeOH, thus leaving the Nitro. No different then getting DCM out of stripper.

    GODISNOWHERE
Shoot Narcs, Not Drugs
 
 
 
 
    Bubbleplate
(Hive Bee)
09-20-02 15:23
No 358605
      Thanks Diggity!  Bookmark   

I knew there had to be an easy answer to this!
I did end up washing the fuel with dH2O. Seems like all the methanol ended up in it. Looks as if the original fuel was about 45% Methanol. So now I have fuel oil which I assume contains all the Nitromethane. Will have to wait for another day to distill...

If they drive God from the earth, we shall shelter Him underground - Dostoevsky
 
 
 
 
    Osmium
(Stoni's sexual toy)
09-20-02 15:38
No 358612
      Just remove everything volatile from the fuel by ...  Bookmark   

Just remove everything volatile from the fuel by distillation, determine the NM content of the distillate, and use the MeOH/NM mixture in your reaction.

I'm not fat just horizontally disproportionate.
 
 
 
 
    Bubbleplate
(Hive Bee)
09-20-02 19:56
No 358680
      Maybe I'll Just Make Some  Bookmark   

From scratch: http://www.orgsyn.org/orgsyn/orgsyn/prepContent.asp?prep=cv1p0401

If they drive God from the earth, we shall shelter Him underground - Dostoevsky
 
 
 
 
    carboxyl
(Hive Bee)
09-22-02 18:51
No 359295
      Like Os said, if your doing a MM, why worry about ...  Bookmark   

Like Os said, if your doing a MM, why worry about a Nitromethane/methanol azeotrope? You're just going to bee adding MeOH anyway!

The above post is purely fictional. Any resemblance to "real-life" is purely coincidental.
 
 
 
 
    baalchemist
(Chef d'Equippe)
09-22-02 22:47
No 359383
      Just check the S.D. properties for purity %, then ...  Bookmark   

Just check the S.D. properties for purity %, then  calculate amount needed to run it based on that. Or just wash the MeOh out since its dirt cheap,,,,,,,

    GODISNOWHERE
Shoot Narcs, Not Drugs
 
 
 
 
    Bubbleplate
(Hive Bee)
09-23-02 05:45
No 359457
      Well Can Report Success  Bookmark   

Went back and washed all the Fuel with dH2O. (Could smell the Methanol in the water)
Dumped washed fuel in still. At 75-80 C. final small amount of methanol came over.  Raised temp. Azeotrope of Nitro/H2O came over. Raised temp again, changed receiving flask. Finally pure Nitro came over. Temp of Oil bath btw, was 110-120 C. Thanks all for suggestions/help!
I think nitro is much safer than people portray it as.


If they drive God from the earth, we shall shelter Him underground - Dostoevsky
 
 
 
 
    slackdaddy
(Stranger)
09-25-02 23:01
No 360674
      I just bought my nitro from a hot-rod shop  Bookmark   

I just bought a gallon of nitromethane from a hot-rod shop.  99+% pure.

One less distillation is worth the small investment.